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Azobisisobutyronitrile → hydroxystyrene (3-acryloxypropyl)trimethylsiloxy Silane

HRID 1355314
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1355314
[C:1]([O:5][CH2:6][CH2:7][CH2:8][SiH2:9][O:10][Si:11]([CH3:14])([CH3:13])[CH3:12])(=[O:4])[CH:2]=[CH2:3].C([O:18][CH:19]=[CH:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)(=O)C.CC(N=NC(C#N)(C)C)(C#N)C>C1COCC1>[OH:18][CH:19]=[CH:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[C:1]([O:5][CH2:6][CH2:7][CH2:8][SiH2:9][O:10][Si:11]([CH3:14])([CH3:12])[CH3:13])(=[O:4])[CH:2]=[CH2:3]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6547AzobisisobutyronitrileHCID 1145762-Phenylvinyl acetateHCID 131723942(3-Acryloxypropyl)trimethylsiloxy silane

Produkt 1

HCID 131723941hydroxystyrene (3-acryloxypropyl)trimethylsiloxy Silane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

5 g (3-acryloxypropyl)trimethylsiloxy silane, 38 g acetoxystyrene and 2.41 g AIBN were dissolved in 128 g THF and charged into a 3-neck flask. The system was then purged with N2 for 30 mins before the temperature was raised to 65° C. The reaction was carried out overnight under N2. On the second day, 100 g methanol and 30 mL 30% ammonia hydroxide were added to the system and the temperature was kept at 60° C. The reaction was carried out overnight under N2. On the third day, the solution was precipitated in 2000 mL water and 20 mL acetic acid. The polymer was collected and dried in vacuum oven overnight at 40° C. The molecular weight was determined by gel permeation chromatography (GPC) to be 7.5K.

Aufarbeitung

  1. additioncharged into a 3-neck flask
  2. customThe system was then purged with N2 for 30 mins before the temperature
  3. additionOn the second day, 100 g methanol and 30 mL 30% ammonia hydroxide were added to the system
  4. customwas kept at 60° C
  5. waitThe reaction was carried out overnight under N2
  6. customOn the third day, the solution was precipitated in 2000 mL water
  7. customThe polymer was collected
  8. customdried in vacuum oven overnight at 40° C

Quellen und Nachweise

ORD-Eintrag
ord-f80cede363f34fd493dd113856f90881
Quelldatensatz
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06586156B2

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